CN105531305A - Thermoplastic article with thermal active agent - Google Patents
Thermoplastic article with thermal active agent Download PDFInfo
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- CN105531305A CN105531305A CN201480050641.6A CN201480050641A CN105531305A CN 105531305 A CN105531305 A CN 105531305A CN 201480050641 A CN201480050641 A CN 201480050641A CN 105531305 A CN105531305 A CN 105531305A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
- A61F13/53—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the absorbing medium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
- A61F13/51—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the outer layers
- A61F13/515—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators characterised by the outer layers characterised by the interconnection of the topsheet and the backsheet
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
- A61F13/00—Bandages or dressings; Absorbent pads
- A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
- A61F13/84—Accessories, not otherwise provided for, for absorbent pads
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/20—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing organic materials
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
- A61L15/225—Mixtures of macromolecular compounds
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/62—Compostable, hydrosoluble or hydrodegradable materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
- B29C65/70—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by moulding
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/18—Plasticising macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/205—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase
- C08J3/21—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase the polymer being premixed with a liquid phase
- C08J3/215—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase the polymer being premixed with a liquid phase at least one additive being also premixed with a liquid phase
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L29/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical; Compositions of hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Compositions of derivatives of such polymers
- C08L29/02—Homopolymers or copolymers of unsaturated alcohols
- C08L29/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2031/00—Other particular articles
- B29L2031/48—Wearing apparel
- B29L2031/4871—Underwear
- B29L2031/4878—Diapers, napkins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
Abstract
An extruded water-soluble article includes a water-soluble polymer having an extrusion temperature of 90 to 150C, a plasticizer, and one or more active agents in a total amount of 0.1 % to 50% by weight of the article. Combining the active agent(s) with a plasticizer prior to melt-blending with the water-soluble polymer prevents phase separation of the active agent and the polymer. Articles include films, fibers, rods, bars and the like. Such articles may be placed in an absorbent article such as a bandage, a medical drape, a wipe, a sheet, a diaper, a pant, or a pad.
Description
As continuation application, this application claims the right of priority of No. 61/884616 application submitted on September 30th, 2013.The full content that No. 61/884616 is applied for is incorporated to herein by reference.
background
The present invention relates to the water insoluble thermoplastic goods extruded adding promoting agent, and for the preparation of the method for these goods.Described promoting agent have to the reality of human skin or the heat effect of perception.Also disclose a kind of exemplary personal care product adding disclosed goods.
Thermal activities agent such as menthol and menthol derivative and relevant cooling compound are widely used in product as in medicine, toothpaste, candy, makeup and sterilant.In recent years, thermal activities agent such as polyvalent alcohol (sugar alcohol) uses as refrigerant in children training trousers, to remind children when urine occurring and polluting.Also consider thermal activities agent to be applied in incontinence and feminine care.
In personal care product is as diaper and liner, add thermal activities agent is not only relatively costly, but also may bring great technological challenge in manufacture course of products, especially when the character of this promoting agent is volatile.Current, thermal activities agent (such as menthol) is powder type (such as through micropackaging).Described powder can be arranged on to form laminating material between two plate substrates, but between described base material and described powder, obtain adhesive bond be challenging.In yes-no decision, described powder can be mixed with wax-like materials and is applied on product component by slit.But, be difficult to the layer obtaining the coating of uniform slit, because some in powder will precipitate in slot coated technological process from preparation.Further, described preparation has the less desirable obvious smell of possibility.Crystallization is compared in thermal activities agent (such as menthol) in packing forms or other non-encapsulated form has at least three shortcomings.Such shortcoming comprises: 1) due to unstable that humidity and temperature susceptibility causes; 2) manufacturing cost of three to five times is exceeded; And 3) responsive to physical force.
When thermal activities agent is added in thermoplastic article, it is intended that 1) manufacture method is that cost is effective, and/or 2) this thermoplastic article can be readily incorporated in personal care product, and/or 3) when thermoplastic article is got wet this thermal activities agent be fast released, and/or 4) this thermal activities agent kept stable before it is strategically placed in induced environment.
summary of the invention
One aspect of the present invention is a kind of water-soluble articles extruded.Described goods comprise the water-soluble polymers of the extrusion temperature with 90 DEG C to 150 DEG C; Fluidizer; And total amount is one or more promoting agents by described product weight 0.1% to 50%.One or more promoting agents described can completely dissolution/dispersion in fluidizer.Meanwhile, one or more promoting agents described and fluidizer form the mixture/solution of homogeneous.The blend of the homogeneous be made up of the mixture/solution of this polymkeric substance of melt blending and homogeneous has the extrusion temperature of 50 DEG C to 125 DEG C.
In another aspect of the present invention, individual absorbing products comprises the absorbent member be clipped between water impervious egative film and the permeable liner of water, and wherein, this liner has the surface outwardly of medial surface and reverse side.Film of the present invention is attached on the surface of the surface outwardly of this liner or the contiguous liner of absorbent member.Described film is made up of such material, and described material comprises the water-soluble polymers of the extrusion temperature with 90 DEG C to 150 DEG C; Fluidizer; And total amount is one or more promoting agents by described product weight 0.1% to 50%.Described activeconstituents is solubilized/dispersible in described fluidizer.Described promoting agent and fluidizer be combined to form uniform mixture/solution.The blend of the homogeneous prepared by the mixture/solution of this polymkeric substance of melt blending and homogeneous has the extrusion temperature of 50 DEG C to 125 DEG C.
In still yet another aspect of the present, a kind of method preparing the goods extruded comprises following three steps.The first, preparation comprises the mixture/solution of thermoplasticity fluidizer and one or more thermal activities agent.The second, form the blend with the homogeneous of the processing temperature of 90 DEG C to 125 DEG C, the blend of described homogeneous comprises described mixture/solution and unbodied water-soluble poval.The blend of described homogeneous comprises one or more thermal activities agent described in 0.1% to 40% by weight.Three, the blend of this homogeneous is extruded with the form of film or fiber.
By considering detailed description and accompanying drawing, further feature of the present invention and aspect will become obvious.
brief description of drawings
By reference to following explanation, appended claims and accompanying drawing, aforementioned and further feature of the present invention and aspect and the mode obtaining them will become more obviously, and the present invention itself will be better understood, wherein:
Fig. 1 is the side-view of an embodiment according to laminating material of the present invention;
Fig. 2 is the side-view of another embodiment according to laminating material of the present invention;
Fig. 3 is the decomposition schematic side view of an exemplary absorbent article.
Reuse Reference numeral to be in the present description and drawings intended to represent same or analogous feature of the present invention or element.
describe in detail
It will be appreciated by the skilled addressee that this discussion is only the explanation to illustrative aspects of the present invention, and be not intended as the restriction of wider aspect of the present invention.
Term " fiber " in the context of the present invention typically refers to meltblown fibers as herein defined or spun-bonded fibre.
Term " laminating material " refer to wherein membrane structure by adhesively or non-adhering be bonded to the material of fibre web as non-woven material or tissue materials.
Term " meltblown fibers " refer to by from multiple carefully, usually rounded die capillaries with the line of melting or filament form molten thermoplastic is expressed into the filament of the thermoplastic material of melting is attenuated and reduce their diameter, usually by the fiber formed in the high velocity air (such as airflow) that heats.Under the particular case of common forming technology, meltblown fibers stream intersects with the one or more flow of material introduced from different directions.Afterwards, meltblown fibers and other optional material are carried by high velocity air and are deposited on collection on the surface.The distribution of the meltblown fibers in formed fibre web and orientation depend on geometry and processing condition.Exemplary melt-blown process is described in each patent and publication, comprise NRL report 4364, " preparation (ManufactureofSuper-FineOrganicFibers) of ultra-fine organic fibre " of V.A.Wendt, E.L.Boone and C.D.Fluharty; NRL reports " device (AnImprovedDeviceFortheFormationofSuper-FineThermoplastic Fibers) for the formation of the improvement of superfine thermoplastic fibre " of 5265, K.D.Lawrence, R.T.Lukas and J.A.Young; And the US3 of the people such as Butin, the US5 of 849, No. 241 people such as United States Patent (USP) and Georger, 350, No. 624 United States Patent (USP)s, it is separately to be incorporated to by reference herein with mode consistent herein.
Term " nonwoven " and " nonwoven web " refer to such material and material web, its have alternating layers but be not with the cognizable Single Fiber of mode alternating layers as knitted fabrics or the structure of filament.Term " fiber " and " filament " commutative use in this article.Nonwoven fabric or fibre web are made up of kinds of processes, such as melt-blown process, spunbond process, air-laid process, hygroscopic water layer process and bonded carded web technique.
Term " personal care absorbent goods " in the context of the present invention or " absorbing products " include but not limited to diaper, diaper pants, training pants, absorbent pants, incontinence product and urine fender etc.
Term " spunbond " and " spun-bonded fibre " refer to such fiber, its by from multiple carefully, usually rounded spinneret capillary pipe extrudes the filament of molten thermoplastic, and reduces the diameter of the filament be extruded subsequently rapidly and formed.
Unless otherwise defined, as use alpha nerein, term " by weight % ", " % by weight ", " wt% " or its derivative should be interpreted as based on dry weight.
In the rest part of this specification sheets, these terms can adopt other language definition.
Present invention relates in general to a kind of water insoluble thermoplastic goods extruded adding thermal activities agent.The thermoplasticity water-soluble polymers making goods has the extrusion temperature of 90 DEG C to 150 DEG C.In article manufacturing process, by fluidizer and mixed with polymers, wherein said fluidizer has one or more thermal activities agent dissolved or be otherwise dispersed in wherein.Meanwhile, promoting agent (multiple actives) and fluidizer form " mixture/solution " of homogeneous." blend " that be combined to form the homogeneous of the extrusion temperature with 50 DEG C to 125 DEG C of the mixture/solution of polymkeric substance and homogeneous.The goods be made up of the blend of homogeneous comprise film, particle, fiber and the fabric made with fiber or other shape extruded.
material
The material manufacturing water insoluble thermoplastic material of the present invention generally comprises polymkeric substance, fluidizer and promoting agent.Other optional material of improving SNR, cost, outward appearance, sensation and/or weather resistance can add this thermoplastic material.
Polymkeric substance: usually, the polymkeric substance used in the present invention is water miscible or water dispersible.Such material comprises one or more the combination in polyvinyl alcohol (PVOH), polyethylene oxide (PEO), polyoxyethylene glycol (PEG), polyacrylic ester (acid), polyacrylamide, polyester or these polymkeric substance.This polymkeric substance has the extrusion temperature of 90 DEG C to 150 DEG C.
The polymkeric substance of expectation is the height amorphous polyethylene alkoxide polymer sold as " NICHIGOG-POLYMER " that can obtain from a SoarusL.L.C., ArlingtonHeights, Illinois.This specific polymkeric substance has 10,000 to 50, the degree of crystallinity of the molecular weight of 000 and 5% to 25% relative low.
On the one hand, multipolymer such as ethylene vinyl acetate (EVA) can combine with matrix polymer.It is considered that, goods of the present invention can comprise by weight up to 30% EVA.
Fluidizer: the effect of fluidizer be a) reduce polymkeric substance coextrusion temperature and b) serve as the carrier be distributed in by thermal activities agent molecule in polymeric matrix.This fluidizer can make inconsistent material and this polymer blending with polymkeric substance.Fluidizer can by dissolving or disperseing to receive thermal activities agent to form the mixture/solution of homogeneous in structure therein.
All suitable fluidizers dissolve selected thermal activities agent as herein described equably.Suitable fluidizer comprises glycerine, PEG-400, PEG-800, PEG-1000 and lower molecular weight poly(propylene oxide)/polyethylene oxide base co-polymer.A kind of fluidizer of expectation is the liquid POLYGYKOL-400 that can derive from ClariantKS.
Typically, fluidizer accounts for the about 0wt.% of the blend of homogeneous to about 40wt.%, is about 5wt.% to about 30wt.% in some embodiments, and is about 10wt.% to about 20wt.% in some embodiments.
Promoting agent: on the one hand, described promoting agent (multiple actives) stimulating human sensory receptor is to be given in and the sensation that changes of occurrence temperature during skin contact.On the other hand, promoting agent (multiple actives) in fact changes the temperature of skin.In either side, according to promoting agent, temperature variation can be described to cooling or heat up.
Promoting agent (multiple actives) mixes with fluidizer as herein described.Suitable promoting agent comprises menthol, menthol derivative, Xylitol, capsaicine, polyvalent alcohol (sugar alcohol), urea, self-heating zeolite or alkali metal compound, magnesio compound as magnesium chloride and magnesium sulfate.Some in these promoting agents are volatile materials (such as menthol or menthol derivative especially have the menthol of the flash-point of 93 DEG C).
On the one hand, promoting agent (multiple actives) exists in the total amount by product weight 0.1% to 50%, or exists in the total amount by product weight 1% to 20%.On the other hand, promoting agent (multiple actives) exists in the total amount by product weight 2% to 10%.
Optional material: in addition to the aforementioned components, still have other additive can join in said composition, as perfume compound, melt stabilizer, dispersing auxiliary (such as tensio-active agent), processing stabilizers, thermo-stabilizer, photostabilizer, ultra-violet stabilizer, antioxidant, heat aging stabilizers, whitening agent, anti blocking agent, static inhibitor, tackiness agent, lubricant etc.
In one aspect of the invention, the water-soluble articles extruded comprise up to by weight 50% thermoplastic starch.The total cost of the goods extruded described in this thermoplastic starch serves as filler to reduce.The described goods extruded can comprise the thermoplastic starch of nearly 30%.A kind of water insoluble thermoplastic starch of expectation is the cellulose base starch obtained by various different plant material, hemicellulose, modified-cellulose (hydroxy alkyl cellulose, ether of cellulose, cellulose ester etc.) etc.When adopting thermoplastic starch, the scope of the amount of material other like this can be the about 1wt.% of the blend of homogeneous to about 50wt.%, be about 5wt.% to about 40wt.% in some embodiments, and be about 10wt.% to about 30wt.% in some embodiments.
Also the uniform dispersion that dispersing auxiliary helps be formed promoting agent/fluidizer can be applied.When applicable, this dispersing auxiliary (multiple dispersing auxiliary) accounts for the about 0.01wt.% of the blend of homogeneous to about 10wt.% usually, be about 0.1wt.% to about 5wt.% in some embodiments, and be about 0.5wt.% to about 4wt.% in some embodiments.
Said composition also can comprise sanitas or preservative system to suppress microbial growth within the period extended.Suitable sanitas can comprise such as alkanols, EDTA (ethylenediamine tetraacetic acid (EDTA)) disodium, edta salt, EDTA lipid acid conjugates, isothiazolinone, benzoic ether (metagin) (such as methyl p-hydroxybenzoate, propylparaben, butyl p-hydroxybenzoate, ethyl p-hydroxybenzoate, p-Hydroxybenzoic acid isopropyl ester, p-Hydroxybenzoic acid isobutyl ester, benzyl p-hydroxybenzoate, Sodium Methyl Hydroxybenzoate and Sodium propyl p-hydroxybenzoate), phenylformic acid, propylene glycol, sorbic ester, urea derivative (such as two Imidurea) etc.Other suitable sanitas comprises those that sold by SuttonLabs, as " Germall115 " (Imidurea), " GermallII " (two Imidurea) and " GermallPlus " (two Imidurea and iodine propine butyl carbonate).Other suitable sanitas is the KathonCG.RTM. of the mixture for methylchloroisothiazandnone and methylisothiazolinone that can obtain from Rohm & Haas; MackstatH66 (can obtain from McIntyreGroup, Chicago, Ill.).Also have another kind of suitable preservative system be 56% propylene glycol, two Imidureas of 30%, the combination of the methyl p-hydroxybenzoate of 11% and the propylparaben of 3%, it can obtain from the international specialty products (InternationalSpecialtyProductsofWayne, N.J) of the Wei En of New Jersey with title GERMABEN.RTM.II.
In order to provide other benefit to human consumer, optional composition can be added to the blend of the mixture/solution of described homogeneous or homogeneous.Such as, the kind of operable optional member can include but not limited to: antioxidant (for product integrity); Cosmetic astringents (for causing sensation of pricking on skin); Tinting material (for giving color for product); Reodorant (for reduce or eliminate unpleasant odor and in order to avoid producing stench on bodily surfaces); Perfume compound (for attracting human consumer); Skin conditioning agent; Shielding medicine for skin (protect skin that is injured or that expose or mucomembranous surface escapes injury or the product of disagreeable stimulation); And antiseptic-germicide.
Expect that goods of the present invention are not using solvent, particularly organic solvent is as obtained when Organic Alcohol (such as ethanol).This can limit the evaporation of any volatile active agent that can join in these goods.
manufacture method
In one aspect of the invention, the method preparing the goods extruded comprises the following steps.The first, the mixture/solution of the homogeneous of preparation thermoplasticity fluidizer and one or more thermal activities agent.The second, by the mixture/solution of homogeneous and combination of polymers being formed the blend of homogeneous.In an embodiment expected, polymkeric substance is amorphous water-soluble vinyl alcohol as described herein.The blend of the homogeneous obtained comprises one or more thermal activities agent.3rd, extrude the blend of described homogeneous to form goods.
Be there is by the blend of the described homogeneous made by the mixture/solution combination of polymkeric substance and homogeneous the extrusion temperature of 50 DEG C to 125 DEG C, or may be 90 DEG C to 125 DEG C.The distribution of this relatively low extrusion temperature prevents being separated of thermal activities agent and is extruding the stage and formed the blend of the homogeneous of at least one polymkeric substance and thermal activities agent (multiple thermal activities agent).In certain aspects, the macroface of crystalline active agent (such as menthol or derivatives thereof) is prevented to be separated.
Extrusion method: composition of the present invention is formed by various ingredients being processed together in melt blending device (such as forcing machine).The mechanical shearing provided by melt blending device and heat make component be blended together not use the efficient way of solvent.Can adopt in the present invention in batches and/or continuous print melt blending technology.Such as, mixing machine/kneader, Ban Buli mixing machine, method labor continuous mixer, single screw extrusion machine, twin screw extruder, roller mill etc. can be utilized.A kind of specially suitable melt blending device is twin screw extruder (such as can derive from ThermoElectricCo., the PRISMUSALABx16 of Inc., NewJersey).
Supply raw material in melt blending device in two stages.Such as, thermal activities agent is dissolved or is otherwise dispersed in form the mixture/solution of homogeneous in this fluidizer, afterwards, this mixture is injected forcing machine in the downstream of polymkeric substance and other optional member as herein described such as starch.
Mixture/the solution of this polymkeric substance and homogeneous forms the blend of homogeneous jointly.Blended under shearing/pressure and temperature that these components can not adversely affect the physicals of thermal activities agent being enough to guarantee abundant mixing (such as more than the fusing point or fusing point of polymkeric substance).Such as, usually at about 50 DEG C to about 150 DEG C, be about 70 DEG C to about 125 DEG C in some embodiments, and in some embodiments for there is melt blending at the temperature of about 80 DEG C to about 99 DEG C.These relatively low processing temperatures prevent any volatilization of promoting agent, decrease the chemical reaction of any thermal initiation simultaneously.
It is expect that following forcing machine is arranged:
Forcing machine extrusion temperature scope: 90-125 DEG C
Temperature setting distribution for the extrusion temperatures of 125 DEG C:
-feed zone 100-110 DEG C
-compression section 110-120 DEG C
-metering zone 120-125 DEG C
-die head 120-130 DEG C
Extrude feeding rate: 2.00-4.00 ppm
Screw speed: 100-250 rotations per minute (rpm)
Once formation, the blend of homogeneous of the present invention can be used to form various ways, as film, fiber, rod, bar or other shape.
film: in a specific embodiment, the blend of homogeneous is separately or be combined with other film formation material and form film.Described film can use in a variety of application, as the carrier of the thermal activities agent of medical product, clothes, absorbing products etc.Described film can have single or multiple lift configuration.Desirably, the thickness of described film is 0.025 millimeter to 0.25 millimeter.Any known technology cause matrix material can be adopted to form film, as the coextrusion of extrusion coated, layer or any routine become layer process.
How periosteum is not formed, described film can optionally along one or more directions orientation to improve film uniformity further and to reduce thickness.Such as, described film can reheat immediately to such temperature, below the fusing point of one or more polymkeric substance of this temperature in film, but enough high so that composition can be made to be stretched or to stretch.When continuous orientation, the film of " softening " is by stretching with the roller of different velocity of rotation or speed, with the stretch ratio making sheet material extend to expectation in longitudinal direction (machine direction).
Described multilayer film can comprise two (2) to eight (8) individual layers, and is three (3) to five (5) individual layers in some embodiments.In an example, described multilayer film has a basic unit and a cortex.This basic unit and/or cortex can comprise thermal activities agent (multiple thermal activities agent).Ratio between this is two-layer can be 20 to 1.
Another example is as shown in FIG. 1 trilamellar membrane 100, and it has the sandwich layer 102 comprising thermal activities agent.Exodermis 104 and 106 can be polyolefine (such as EVA).Ratio between layer can be the cortex of the sandwich layer of 60% to 40% and two combinations of 90% to 10%.Such as, sandwich layer can up to about 30% of the total thickness of multilayer film, up to about 40%, up to about 50%, up to about 60% or up to 70%.Each cortex can up to about 15% of multilayer film total thickness or up to about 25% or up to about 35%.Described cortex can have different thickness relative to each other.
This film is individual layer or multilayer, can reel on winding roller and store.Various other possible processing and/or correction step known in the art can be carried out, as the lamination of cutting, process, pore-forming, printed pattern or film and other layer (such as nonwoven web material).
On the one hand, the water-solubility membrane extruded has 5 grams every square metre (gsm) basic weight to 500gsm.On the other hand, this water-solubility membrane has the basic weight of 20gsm to 200gsm.
On the one hand, according to Elongation test of the present invention, the water-solubility membrane extruded has the tensile strength of 0.5MPa to 50MPa.On the other hand, according to identical test, this film has the tensile strength of 1MPa to 25MPa.
On the one hand, as determined by dissolving test of the present invention, the water-solubility membrane extruded has the dissolving speed of 5 seconds to 30 minutes.On the other hand, the water-soluble articles film extruded described in has the dissolving speed of 30 seconds to 5 minutes as determined by same test.
On the one hand, according to Elongation test of the present invention, described in the water-solubility membrane extruded present 5% to 500% elongation.On the other hand, according to identical test, this film presents the elongation of 10% to 100%.
goods: the blend of homogeneous of the present invention can also for the formation of the goods of other type.On the one hand, the water-soluble articles extruded described in has the rod that circle or ellipse extrude profile.On the other hand, the water-soluble articles extruded described in is the rod that Polygons (such as trilateral is to the decagon) geometry with three to ten sides extrudes profile.This rod can be cut into particle for following process.
See Fig. 2, laminating material 20 is by being expressed into the blend 24 of homogeneous on carrier substrate 22 to form bonding between which to be formed.This carrier substrate 22 can be non-woven material, weaving material, Mierocrystalline cellulose fibre web etc.Such laminating material can be used as sheet material or be used as the assembly of absorbing products as described herein, and described absorbing products is as bandage, diaper, liner, medical coverlet and trousers.
On the one hand, this laminating material 20 can be used as being sold to human consumer with drying regime and the towel soaked by human consumer.Human consumer can be ultimate consumer.This offers at least the advantage reducing transportation cost.
application
Absorbing products: film of the present invention is particularly suitable for using in absorbing products." absorbing products " typically refers to any goods that can absorb water or other fluid.The example of some absorbing products includes but not limited to personal care absorbent goods, as diaper, training pants, absorbent pants, incontinence articles, feminine hygiene (such as sanitary towel, protection pad etc.), swimming suit, baby's towel etc.; Medical absorbent products, as clothes, windowing material, mat, mattress, bandage, absorptivity coverlet and medical towel; Food and beverage sevice towel; Clothing item; Etc..Some examples of such absorbing products at the US5 of the people such as DiPalma, 649, No. 916; The US6 of Kielpikowski, 110, No. 158; The US6 of the people such as Blaney, has description in 663, No. 611 United States Patent (USP)s, is incorporated to by reference herein by its full content for all objects.The goods still having other suitable at the US4 of the people such as the application of US2004/0060112A1 U.S. Patent Publication and Damico of the people such as Fell, 886, No. 512; The US5 of the people such as Sherrod, 558, No. 659; The US6 of the people such as Fell, 888, No. 044; And the US6 of the people such as Freiburger, there is description in 511, No. 465 United States Patent (USP)s, for all objects, its full content is incorporated to herein in this by reference.The materials and process being suitable for being formed such absorbing products is well known to those skilled in the art.
The present invention is will be better understood with reference to Multi-instance provided in this article.
Exemplary absorbent article: see Fig. 3, in one aspect of the invention, individual's absorbing products 30 comprises absorbent member 32, this absorbent member 32 is clipped between water impervious egative film 34 and the permeable liner 36 of water, and wherein liner 36 has the surface 40 outwardly of medial surperficial 38 and reverse side.Film 41 of the present invention is attached to the surface 42 of the surface 40 outwardly of this liner or the contiguous liner 36 of absorbent member 32.Desirably, film 41 directly contacts with liner 36.When multilayer film is used as film 41, layer this liner 36 contiguous comprising the promoting agent of maximum can more easily leach through liner 36 with the Body contact with wearer to make promoting agent.
As described, film 41 is made up of such material, and this material comprises the water-soluble polymers of the extrusion temperature can with 90 DEG C to 150 DEG C; Fluidizer; And total amount is one or more thermal activities agent by product weight 0.1% to 50%.
experimental data
Twin screw extruder (PRISMUSALABx16 that can buy from ThermoElectricCo., Inc.) is used to prepare the membrane sample of the coextrusion comprising menthol.The specification of this forcing machine is as follows:
The screw rod of 16 mm dias
L/D=40 (L=640 millimeter)
10 heating zone+die heads
Top speed=1000rpm
Peak pressure=100bar
Peak torque=24mN:
Following forcing machine is adopted to arrange preparation experiment film:
Flush joint die width: 152.40mm (6 ")
Flush joint die head height (controlling diaphragm thickness): 0.127mm (0.010 ")
The film of this coextrusion comprises menthol (99% purity, crystalline form, from Sigma-AldrichCorp., St.Louis, MO).The menthol of 100 grams and the polyoxyethylene glycol (Polyglykol)-400 liquid (from Clariant, Charlotte, NC.) of 400g mix.In order to prepare the homogeneous solution of mixture, this mixture heats menthol is dissolved completely in an oven at 60 DEG C.(menthol/polyoxyethylene glycol (polyglykol) solution of the homogeneous as desired, obtained is not separated after being arranged in the baking oven at 25 DEG C storage of spending the night).
This forcing machine intake zone is heated to 110 DEG C, and forcing machine district 2-9 is below heated to 125 DEG C, and die head is heated to 130 DEG C.
Amorphous polymer, i.e. the G-polymkeric substance from Nippon-Goshie as herein described; And from thermoplastic starch, the thermoplastic starch glucose-800 of ChemstarProductsCompany, Minneapolis, MN, be fed in forcing machine feed zone with 1.0 gram/minute.Menthol/the polyglycol solution of homogeneous is also pumped in forcing machine feed zone with the speed of 1.0 gram/minute.The film of 2-5 mil thick is extruded under 150-200rpm.
Cooling sensory test:
The cooling sensation provided by menthol film is subjectively determined as follows.The first, it is in the water of about 23 DEG C and the forearm subsequently this film being attached to people's tested object that the film (as above preparing) containing 2% menthol is immersed in temperature.Laboratory condition be about 50% relative humidity, at 23 DEG C.
Tested object feels in being reported in 2 minutes after being placed on forearm by film that cooling is felt.The cooling persistence of sensation 15-30 minute of report.Control sample not containing menthol does not provide any cooling to feel.
Dissolve test:
Dissolve the process that test is the estimated value determining the dissolution time of polymeric film in deionized water or physiological saline.ASTM standard method of test D5226-98 " standard practices for dissolve polymer material " uses together with any test variance hereinafter described.This test is for 1) relative dissolution time of more dissimilar polymkeric substance, and 2) observe and the additive of polymer blending and/or the effect of other promoting agent.Although have recorded the time of each Test code, this test is not quantitative, because people visually must determine the terminal that film dissolves.
1. sample preparation
A. with die head and pressing machine, sample polymer film is cut into the bar of 2.54 centimetres x15.24 centimetre (1 inch of x6 inch).
B. three samples are cut for each membrane sample.
2. Setup Experiments and process
A. deionized water or physiological saline put into 1L glass beaker and be heated to 37 DEG C in hot water bath to help the stoppage time reduced between sample testing.
B. the quality of each is measured with standard balance.
C. expect that the quality of film and the mass ratio of medium are 0.5%.Therefore, the appropriate mass of medium is gone out based on the Mass Calculation measured.
D., after medium is adjusted to room temperature, balance is used to obtain the medium of appropriate mass.This medium is placed in 250 milliliters of glass beakers with the magnetic stirring bar of 1.5 inches.
E. subsequently beaker is placed on the VWR hot plate/agitator with feedback temperature meter.Check that the temperature of medium is to guarantee that medium is at 37 DEG C afterwards.Stir speed (S.S.) is set to 100rpm.
F. after, film doubling (sticking on the side of beaker to prevent film) is placed on the water surface.At this time start timing.
G. film in solution is tightly monitored subsequently to observe the dissolution process of film and to determine the terminal of dissolving.
H. terminal is mainly through staying the size of complete film in the solution to determine.
I. dissolve 90% the standard being set as terminal.When most of macrobead is dissolved, record terminal.
Ii. target is the surface-area of 6 square inches to about 0.6 square inch.If this film is rolled into ball, then this means the radius of about 6.4 millimeters.
Iii. the turbidity of water or normal saline solution is secondary cause.
1. many films are rice white or black, and cause this solution to become muddy when dissolving.But turbid solution contributes to determining terminal.
I. accuracy testing
I. because terminal is visually assessed, therefore carry out checking to determine accuracy.Once determine terminal, continue the test period of monitoring coating solution two double-length, to guarantee that this film can not continue to dissolve significantly.Such as, if the terminal of film is measured as 45 seconds, then continue this film of monitoring by 90 seconds to guarantee can not occur to dissolve further and the accuracy helping raising to test and repeatability.
3. data analysis
A. record the dissolution time result of each sample and calculating mean value for the statistical of different blend polymers.
As above the menthol film prepared has the dissolution rate of about 5 seconds.
Elongation test: before testing, make at first film sample 75 °F and 50% relative humidity under adapt to 24 hours.Afterwards, tensile strength values is determined according to ASTM standard D882-10.
Adopt constant speed extended stretching testing machine as MTSSynergie200 mechanical testing machine (MTSSystemCo., MN, the U.S.).Select suitable load sensor, to make, measured value falls in the scope of the 10-90% of full scale load.
According to ASTM standard method of test D6287 " for cutting the standard practices of film and sheet test sample ", specimen size is 101.6 millimeters of x9.525 millimeters (4 " x3/8 ").
Sample is remained between coating glue clamp that gauge length is 50.8 millimeters (2 inches).Sample is stretched until rupture under the pinblock speed of about 508 mm/min (20 inch per minute clock).Test at least 16 samples, at least 8 are passed through to apply testing load in the machine direction of sample, and at least 8 samples are tested by the transversely applying testing load at sample.Young's modulus, peak load, peak stress, elongation (percent strain during fracture) and unit volume energy-to-break (overall area under stress-strain curve) can be obtained from result.
Claims (20)
1. the water-soluble articles extruded, it comprises:
There is the water-soluble polymers of the extrusion temperature of 90 DEG C to 150 DEG C; Fluidizer; And total amount is one or more thermal activities agent by described product weight 0.1% to 50%, one or more promoting agents wherein said can completely dissolution/dispersion in described fluidizer;
The combination of one or more thermal activities agent wherein said and fluidizer is the mixture/solution of homogeneous; And
The blend wherein comprising the homogeneous of the mixture/solution of polymkeric substance and homogeneous has the extrusion temperature of 50 DEG C to 125 DEG C.
2. the water-soluble articles extruded according to claim 1, wherein said polymkeric substance is selected from polyvinyl alcohol (PVOH), polyethylene oxide (PEO), polyoxyethylene glycol (PEG), polyacrylic ester (acid), polyacrylamide, polyester, thermoplastic starch, polyolefin copolymer and combination thereof.
3. the water-soluble articles extruded according to claim 1 and 2, wherein said fluidizer is selected from glycerine, PEG-400, PEG-800, PEG-1000 and lower molecular weight poly(propylene oxide)/polyethylene oxide base co-polymer.
4. the water-soluble articles extruded according to claim 1 and 2, wherein said polymkeric substance is amorphous ethylene alcohol matrix.
5. the water-soluble articles extruded according to claim 1 and 2, wherein said extrusion temperature is 90 DEG C to 125 DEG C.
6. the water-soluble articles extruded according to claim 1 and 2, the total amount of one or more thermal activities agent wherein said is the weighing scale 1% to 20% by described goods.
7. the water-soluble articles extruded according to claim 1 and 2, its also comprise up to by weight 50% thermoplastic starch.
8. the water-soluble articles extruded according to claim 1 and 2, its also comprise up to by weight 30% ethylene vinyl acetate.
9. the water-soluble articles extruded according to claim 1, wherein said goods are single or multiple lift films.
10. the water-soluble articles extruded according to claim 9, wherein said film has as dissolved by of the present invention the dissolving speed of 5 seconds to 30 minutes tested and determine.
11. water-soluble articles extruded according to claim 9, wherein said film has the basic weight of 5 grams every square metre to 500 grams every square metre.
12. water-soluble articles extruded according to claim 9, wherein said film has the elongation according to 5% to 500% of Elongation test of the present invention.
13. water-soluble articles extruded according to claim 1 and 2, one or more promoting agents wherein said are menthol, its menthol derivative or its combination.
14. water-soluble articles extruded according to claim 1 and 2, when one or more thermal activities agent wherein said are formed at skin contact, stimulating human sensory receptor or change the temperature of skin.
15. water-soluble articles extruded according to claim 1 and 2, one or more thermal activities agent wherein said comprise temperature reagent, and described temperature reagent is selected from menthol, menthol derivative, Xylitol, capsaicine, polyvalent alcohol, urea, self-heating zeolite or alkali metal compound, magnesium chloride, magnesium sulfate and combination thereof.
16. 1 kinds of individual absorbing products, it comprises:
Be clipped in the absorbent member between water impervious egative film and the permeable liner of water, wherein this liner has the surface outwardly of medial surface and reverse side; And
Be attached to the film on the surface of the surface outwardly of this liner or the contiguous liner of absorbent member, wherein said film comprises: the water-soluble polymers with the extrusion temperature of 90 DEG C to 150 DEG C; Fluidizer; And total amount is one or more thermal activities agent by described product weight 0.1% to 50%, one or more thermal activities compositions wherein said are solubilized/dispersible in described fluidizer; The combination of one or more thermal activities agent wherein said and fluidizer is the mixture/solution of homogeneous; And the blend wherein comprising the homogeneous of the mixture/solution of polymkeric substance and homogeneous has the extrusion temperature of 50 DEG C to 125 DEG C.
17. individual absorbing products according to claim 16, wherein said individual absorbing products is bandage, medical coverlet, towel, sheet, diaper, trousers or liner.
The method of 18. 1 kinds of goods preparing to extrude, it comprises the following steps:
A) preparation comprises the mixture/solution of thermoplasticity fluidizer and one or more thermal activities agent;
B) blend with the homogeneous of processing temperature of extruding with 90 DEG C to 125 DEG C is formed, the blend of described homogeneous comprises described mixture/solution and amorphous water-soluble polyvinyl alcohol, and the blend of wherein said homogeneous comprises one or more thermal activities agent described in 0.1% to 40% by weight; And
C) blend of described homogeneous is extruded to form film.
19. methods according to claim 18, the blend of wherein said homogeneous can directly be expressed on carrier substrate, is formed and bond between the blend and carrier substrate of homogeneous.
20. methods according to claim 18 and 19, wherein one or more second promoting agents are coextruded together with the blend of described homogeneous.
Applications Claiming Priority (3)
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| US201361884616P | 2013-09-30 | 2013-09-30 | |
| US61/884616 | 2013-09-30 | ||
| PCT/US2014/057729 WO2015048450A1 (en) | 2013-09-30 | 2014-09-26 | Thermoplastic article with thermal active agent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105531305A true CN105531305A (en) | 2016-04-27 |
Family
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|---|---|---|---|
| CN201480050641.6A Pending CN105531305A (en) | 2013-09-30 | 2014-09-26 | Thermoplastic article with thermal active agent |
Country Status (9)
| Country | Link |
|---|---|
| US (1) | US20160235601A1 (en) |
| EP (1) | EP3052552B1 (en) |
| KR (1) | KR20160054020A (en) |
| CN (1) | CN105531305A (en) |
| AU (1) | AU2014324820B2 (en) |
| BR (1) | BR112016006517B1 (en) |
| MX (1) | MX367400B (en) |
| RU (1) | RU2638397C2 (en) |
| WO (1) | WO2015048450A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109414341A (en) * | 2016-06-27 | 2019-03-01 | 尤妮佳股份有限公司 | Warming piece |
| CN109923172A (en) * | 2016-11-30 | 2019-06-21 | 金伯利-克拉克环球有限公司 | Material that is thermoplastic injection-molded and can breaking up |
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| US7910797B2 (en) | 2006-09-18 | 2011-03-22 | The Procter & Gamble Company | Absorbent articles having a sensation aspect |
| US10562281B2 (en) * | 2011-08-02 | 2020-02-18 | Kimberly-Clark Worldwide, Inc. | Cooling signal device for use in an absorbent article |
| EP3990686B1 (en) * | 2019-06-26 | 2024-01-03 | 3M Innovative Properties Company | Method of making a nonwoven fiber web, and a nonwoven fiber web |
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Also Published As
| Publication number | Publication date |
|---|---|
| RU2016114230A (en) | 2017-10-18 |
| RU2638397C2 (en) | 2017-12-13 |
| EP3052552A4 (en) | 2017-05-03 |
| WO2015048450A1 (en) | 2015-04-02 |
| MX2016004004A (en) | 2016-06-02 |
| MX367400B (en) | 2019-08-15 |
| US20160235601A1 (en) | 2016-08-18 |
| EP3052552A1 (en) | 2016-08-10 |
| BR112016006517B1 (en) | 2021-08-17 |
| BR112016006517A2 (en) | 2017-08-01 |
| KR20160054020A (en) | 2016-05-13 |
| AU2014324820B2 (en) | 2018-02-01 |
| EP3052552B1 (en) | 2019-07-31 |
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Application publication date: 20160427 |